1,3-Diethyl 2-oxopropanedioate → Ethyl 6,7-dichloro-3-hydroxyquinoxaline-2-carboxylate

HRID 2057364

反応式

HRID 2057364 の反応式
[Cl:1][C:2]1[C:7]([Cl:8])=[CH:6][C:5]([NH2:9])=[C:4]([NH2:10])[CH:3]=1.O=[C:12]([C:18](OCC)=[O:19])[C:13]([O:15][CH2:16][CH3:17])=[O:14]>C(O)C>[Cl:1][C:2]1[CH:3]=[C:4]2[C:5](=[CH:6][C:7]=1[Cl:8])[N:9]=[C:12]([C:13]([O:15][CH2:16][CH3:17])=[O:14])[C:18](=[O:19])[NH:10]2

参加物

4

反応物 2

HCID 691051,3-Diethyl 2-oxopropanedioateHCID 792974,5-Dichloro-1,2-phenylenediamine

生成物 1

HCID 6320212Ethyl 6,7-dichloro-3-hydroxyquinoxaline-2-carboxylate

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of 17.7 g. of 4,5-dichloro-o-phenylenediamine in 200 ml. of anhydrous ethanol was prepared. A 17.4 g. batch of diethyl 2-ketomalonate were added to this solution and the mixture was heated to refluxing temperature for about 17 hours. The volatile constituents were removed by evaporation in vacuo. Recrystallization of the residue from ethanol yielded 20 g. of ethyl 6,7-dichloro-3,4-dihydro-3-oxo-2-quinoxaline carboxylate formed in the above reaction, melting in the range 226°-227° C.

後処理

  1. temperaturethe mixture was heated
  2. temperatureto refluxing temperature for about 17 hours
  3. customThe volatile constituents were removed by evaporation in vacuo
  4. customRecrystallization of the residue from ethanol
  5. customyielded 20 g

出典と根拠

ORDレコード
ord-deb283faf74749fbb825ea8679c15516
出典データセット
uspto-grants-1980_07
特許番号
US04210647

関連ノート

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